Hard bituminous material



g 1 V NITED v STATE Patented A r. 30, 1940 HARD BITUMINOUS MATERIAL Kenneth QLaughlin, Baton Rouge, La., assignor to Standard Oil Devel poration of Delaware No Drawing.

opment Company, a 001'- Application March 31; 1936, Serial No. 71,925 1 l 1 Claim. (or. 196-452) This invention relates to hardbituminous material and a process for preparing the same. More particularly it relates to high meltingaS- phalts having a definite change in penetration with temperature and being especially suitable for the manufacture of molded asphaltic products generally and electric storage battery box compound specifically. The invention will be fully understood from the following description.

Asphalts may be obtained from petroleum in a variety of different ways. The particular method used depends very largely upon the use to which the asphalt is to be put. v Asphalts to be Test N0. D36-26 f the A. .S. T. M.

used for electric storage battery box compound and molded asphaltic products generally must meet certain specifications defined by the manufacturersof such products. These specifications I are met at the present time by compounding natural asphalt (Gilsonite) with various petro- .20

leum asphalts. These asphalt blends are unsatisfactory for battery box manufacture in some respects and the manufacturers have drawn up a set of specifications for an ideal bitumen to be used in compounding battery boxes.

Thus an asphalt to be used for battery box compound should have a penetration between 14 and 18 at 150 F./100 grams/ secs. as del termined by Test No. D5-25 of theAmerican Society for Testing Materials (A. S. T. M.)..

The susceptibility factor should be between27 and as calculated by the following formula:

Penetration @150/100g/5 sees. Penetration @l85/50g/5 secs. Penetration @1l5/200g/5 sccs. Penetration @150/l00g/5 scesl The softening point should be above about 260 F. as determined by the ring and ball method,

. The ductility should behigh, that is about 35 to centimeters at 185 F. at the rate of 5 cm./min. as determined by Test No. D1l3-35 of the A. S. T. M. r

The present invention is directed to a new process for obtaining from petroleum, asphalts having the above characteristics.

It is already knownthat asphalt may be precipitated from petroleum and fractions thereof by diluting the same with liquefied normally gaseous hydrocarbons at normal or slightly higher temperatures. It has been found, however, that theasphalts so produced do not have the required penetration, susceptibility and ductility characteristics to adapt them for use as battery box compound and molded asphaltic products.

It has now been found that if a petroleum residue is diluted with a liquefied hydrocarbon having 4 carbon atoms and the mixture heated to a high temperature, the asphalt so precipitated will havethe desired characteristics referred to above. In effect this method may be said to conslst in the high temperature butane precipitation of asphalt from petroleum. 'I'hemethod is car: ried out as follows:

A petroleum residue containing asphalt mixed with from 4 to 10, preferably about 6 to 8,

Other hydrocare L volumes of liquefied butane. bon's having 4 carbon atoms such as isobutane, 'butylene, and isobutylene may; of course, also be used. The mixture is heated to a temperature between 150 and 300 F., preferably about 200 F., and pressure .is maintained sufficient to retain the butane in liquidphase atthe tempera ture of working The mixture is allowed to stand at substantiallythe same high temperature un: til the asphaltic layer .has settled out and it is ,then drawn on. It is found that the asphalt when so precipitated comes down in a iluidcondition which greatly facilitates efficient mixing and settling.

It will be understood that the precipitation may be carried out in a batch manner as indicated above, or in a continuous counter-current manner either in a tower or in a series of sep arate but inter-connected stages. The apparatus for the counter-current treating may be substantially the same as that usually employed in such processes, but special provision must, of course, be made for heating the mixture and it is preferable to insulate the settling chamber to prevent undue heat losses. l

The following example illustrates the applica tionof the process:

A Lago (Venezuela) crude petroleum is distilled to about 17.5% bottoms having a penetration of 180 to 200 at 77 F./g/secs. .The bottoms is mixed with about '7 volumes of butane and the mixture heated to a temperature of about 200 F. where it is maintained until the precipitated. asphalt has settled. The asphalt layer which is liquid is drawnoii and the butane is stripped therefrom with natural gas at a temperature of about 400 F. The asphalt so obtained has the following characteristics:

Yield on bottoms "percent" 40 Softening point (ball and ring) "F 263 Flash point, Cleveland 0. (3., "F a 560 Ductility 150 F.,5 cm./min 9 Ductility 185 5 cm./min 38 Susceptibility factor 33.7 Penetration 77 F./100g./5 se'c 0 Penetration (1) F./200g./5 sec 11 Penetration F./100g./5 sec 17.5 Penetration F./50g./5 sec 31 i r Soluble in CS2 99.80 Insoluble in 86 naphtha 77.2 Fixed carbon s 36.2 Specific gravity 77 F 1.006 Volatile 5 hrs. 500 F. 50 grams 0.96 

